UPLC-MS/MS法同时检测人血浆中唑吡坦、右佐匹克隆和扎来普隆的方法研究
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篇名: UPLC-MS/MS法同时检测人血浆中唑吡坦、右佐匹克隆和扎来普隆的方法研究
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摘要: 目的:建立快速、准确、可同时检测人血浆中唑吡坦、右佐匹克隆和扎来普隆的分析方法。方法:血浆样品经液-液萃取后,以卡马西平为内标,采用超高效液相色谱-串联质谱法检测。色谱柱为Waters ACQUITY UPLC HSS T3,流动相为0.1%氨水-乙腈(梯度洗脱),流速为0.2 ml/min,柱温为40 ℃,进样量为5 μl。采用电喷雾离子源,以多反应监测方式进行正离子扫描,用于定量分析的离子对分别为m/z 308.2→263.1(唑吡坦)、m/z 389.3→245.0(右佐匹克隆)、m/z 306.2→236.1(扎来普隆)、m/z 237.3→151.2(内标)。结果:唑吡坦、右佐匹克隆、扎来普隆血药浓度分别在0.02~20.00、0.50~20.00、0.02~20.00 ng/ml范围内线性关系良好(r分别为0.990 1、0.996 8、0.991 7),定量下限分别0.02、0.50、0.02 ng/ml,检测限分别为0.01、0.20、0.01 ng/ml;日内、日间RSD<15%,提取回收率为88.9%~106.5%,基质效应为94.8%~106.3%。结论:该方法简便、快速、灵敏度高、专属性好,可用于人血浆中唑吡坦、右佐匹克隆和扎来普隆的同时检测。
ABSTRACT: OBJECTIVE: To develop a method for rapid, accurate and simultaneous determination of dexzopiclone, zolpidam and zaleplon in human plasma. METHODS: After the plasma sample was processed by liquid-liquid extraction, UPLC-MS/MS was established to detect plasma sample with carbamazepine as internal standard. The separation was performed on a Waters ACQUITY UPLC HSS T3 column with mobile phase composed of 0.1% ammonium solution-acetonitrile (gradient elution) at flow rate of 0.2 ml/min. The column temperature was set at 40 ℃, and sample size was 5 μl. The detection was performed by multiple reaction monitoring (MRM) via electrospray ionization (ESI) source in positive mode. The mass transition ion-pairs were as follows: m/z 308.2→263.1(zolpidem), m/z 389.3→245.0(dexzopiclone), m/z 306.2→236.1(zaleplon), m/z 237.3→151.2(internal standard). RESULTS: The linear range of zolpidem, dexzopiclone and zaleplon were 0.02-20.00, 0.50-20.00, 0.02-20.00 ng/ml, respectively (r=0.990 1,0.996 8, 0.991 7). LLOQ of them were 0.02, 0.50, 0.02 ng/ml, and detection limit were 0.01, 0.20, 0.01 ng/ml. RSDs of intra-day and inter-day were all lower than 15%; extraction recovery were 88.9%-106.5%; matrix effect were 94.8%-106.3%. CONCLUSIONS: The method is simple, rapid, sensitive and specific, and it can be used for simultaneous determination of zaleplon, zolpidem and dexzopiclone in human plasma.
期刊: 2016年第27卷第23期
作者: 魏欣,安静,吴茵,董占军,范理菊,白万军
AUTHORS: WEI Xin,AN Jing,WU Yin,DONG Zhanjun,FAN Liju,BAI Wanjun
关键字: 超高效液相色谱-串联质谱法;唑吡坦;右佐匹克隆;扎来普隆;检测
KEYWORDS: UPLC-MS/MS; Zolpidem; Dexzopiclone; Zaleplon; Determination
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